1,4-Dioxane hydrochloride → HCID 178509379, 화합물

HRID 489449노트

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HRID 489449 반응식
[N:1]1[O:2][N:3]=[C:4]2[C:9]([CH:10]3[C:15]([C:16]#[N:17])=[C:14]([CH:18]4[CH2:27][CH2:26][CH2:25][CH2:24][C:19]54OCC[O:20]5)[NH:13][C:12]4=[N:28][NH:29][CH:30]=[C:11]34)=[CH:8][CH:7]=[CH:6][C:5]=12.O1CCOCC1.Cl>CO>[N:1]1[O:2][N:3]=[C:4]2[C:9]([CH:10]3[C:15]([C:16]#[N:17])=[C:14]([CH:18]4[CH2:27][CH2:26][CH2:25][CH2:24][C:19]4=[O:20])[NH:13][C:12]4=[N:28][NH:29][CH:30]=[C:11]34)=[CH:8][CH:7]=[CH:6][C:5]=12

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 178509375HCID 178509375, 화합물

생성물 1

HCID 178509379HCID 178509379, 화합물수율 2.2%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

To a solution of 4-(2,1,3-Benzoxadiazol-4-yl)-5-cyano-4,7-dihydro-6-(1,4-dioxa-spiro[4,5]decan-6-yl)-2H-pyrazolo[3,4-b]pyridine (1.0 g) in methanol (30 mL) was added 4N HCl dioxane solution (6.0 mL) at room temperature and the mixture was heated at 60° C. for two hours. After alkalification with sodium bicarbonate, the mixture was extracted with chloroform. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate (1:1)) to give the title compound (20 mg) as colorless crystals.

후처리

  1. extractionAfter alkalification with sodium bicarbonate, the mixture was extracted with chloroform
  2. customThe solvent was evaporated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate (1:1))

출처 및 근거

ORD 기록
ord-c44be7b8f19f4fa5a7c62c9661cbdc7a
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06977262B2

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